#------------------------------------------------------------------------------
#$Date: 2022-02-04 21:56:19 +0200 (Fri, 04 Feb 2022) $
#$Revision: 272734 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061092.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7061092
loop_
_publ_author_name
'Firdoos, Tahira'
'Kumar, Pretam'
'Radha, Anu'
'Gomila, Rosa M.'
'Frontera, Antonio'
'Sood, Puneet'
'Pandey, Sushil K.'
_publ_section_title
;
 An insight into triel bonds in O,O′-diarylphosphorodithioates of
 thallium(i): experimental and theoretical investigations
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              832
_journal_page_last               843
_journal_paper_doi               10.1039/D1NJ04852J
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C18 H22 O2 P S2 Tl'
_chemical_formula_sum            'C18 H22 O2 P S2 Tl'
_chemical_formula_weight         569.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-07-02
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2021-09-13 deposited with the CCDC.	2021-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                107.092(11)
_cell_angle_beta                 95.785(10)
_cell_angle_gamma                90.443(8)
_cell_formula_units_Z            2
_cell_length_a                   8.4373(8)
_cell_length_b                   9.6672(9)
_cell_length_c                   12.6725(19)
_cell_measurement_reflns_used    2393
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      28.1060
_cell_measurement_theta_min      2.2170
_cell_volume                     982.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 120.00   1.00    4.46    --   26.84 178.00  90.00   85
  2  ω     28.00 107.00   1.00    4.46    --   26.84  37.00 -60.00   79
  3  ω    -54.00  67.00   1.00    4.46    --   26.84 -77.00  60.00  121
  4  ω    -47.00  65.00   1.00    4.46    --   26.84 -57.00 150.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0193326000
_diffrn_orient_matrix_UB_12      0.0131258000
_diffrn_orient_matrix_UB_13      0.0552004000
_diffrn_orient_matrix_UB_21      0.0784940000
_diffrn_orient_matrix_UB_22      -0.0168244000
_diffrn_orient_matrix_UB_23      0.0165883000
_diffrn_orient_matrix_UB_31      0.0247899000
_diffrn_orient_matrix_UB_32      0.0737984000
_diffrn_orient_matrix_UB_33      0.0121225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_unetI/netI     0.1221
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5647
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.064
_refine_diff_density_max         4.812
_refine_diff_density_min         -3.106
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0897P)²+26.2224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2222
_reflns_number_gt                3316
_reflns_number_total             4026
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj04852j2.cif
_cod_data_source_block           tl_4iso_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7061091--7061092.cif.'
_cod_database_code               7061092
_chemical_oxdiff_formula         'C36 H42 O4 P2 S4 Tl2'
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C1AA(H1AA), C9(H9), C15(H15), C17(H17), C20(H20), C22(H22), C26(H26), C30(H30)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C2AA(H2AA,H2AB,H2AC)
;
_olex2_date_sample_data_collection 2021-05-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.940
_oxdiff_exptl_absorpt_empirical_full_min 0.674
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Tl2 Tl 0.22521(7) 0.36228(6) 0.41875(5) 0.0310(2) Uani 1 d . . .
S2 S 0.3631(5) 0.6173(4) 0.6033(3) 0.0254(8) Uani 1 d . . .
S4 S 0.0454(4) 0.6556(4) 0.4357(3) 0.0251(8) Uani 1 d . . .
P5 P 0.2413(4) 0.7428(4) 0.5316(3) 0.0187(7) Uani 1 d . . .
C2 C -0.296(2) 1.1741(18) 0.9482(15) 0.036(4) Uani 1 d . . .
H2A H -0.1907 1.2094 0.9821 0.053 Uiso 1 calc . . GR
H2B H -0.3697 1.1987 1.0032 0.053 Uiso 1 calc . . GR
H2C H -0.3269 1.2175 0.8906 0.053 Uiso 1 calc . . GR
O3 O 0.2062(12) 0.8980(11) 0.6194(10) 0.027(2) Uani 1 d . . .
C5 C 0.7302(19) 0.5809(18) 0.1142(14) 0.029(3) Uani 1 d . . .
H5 H 0.6690 0.5013 0.0584 0.035 Uiso 1 calc . . R
C8 C 0.762(2) 0.696(2) 0.0584(16) 0.040(4) Uani 1 d . . .
H8A H 0.8165 0.7789 0.1120 0.060 Uiso 1 calc . . GR
H8B H 0.6628 0.7248 0.0286 0.060 Uiso 1 calc . . GR
H8C H 0.8273 0.6580 -0.0006 0.060 Uiso 1 calc . . GR
O10 O 0.3547(13) 0.8201(11) 0.4678(10) 0.028(2) Uani 1 d . . .
C1 C 0.891(2) 0.520(2) 0.1464(15) 0.039(4) Uani 1 d . . .
H1A H 0.9370 0.4690 0.0803 0.059 Uiso 1 calc . . GR
H1B H 0.8738 0.4557 0.1892 0.059 Uiso 1 calc . . GR
H1C H 0.9626 0.5989 0.1897 0.059 Uiso 1 calc . . GR
C4 C -0.2969(18) 1.0138(18) 0.8998(13) 0.025(3) Uani 1 d . . .
H4 H -0.2737 0.9709 0.9604 0.030 Uiso 1 calc . . R
C0AA C -0.1632(17) 0.9756(16) 0.8226(13) 0.023(3) Uani 1 d . . .
C1AA C -0.0467(17) 0.9916(16) 0.6583(13) 0.023(3) Uani 1 d . . .
H1AA H -0.0528 1.0227 0.5952 0.028 Uiso 1 calc . . R
C9 C -0.1670(19) 1.0225(17) 0.7305(14) 0.027(3) Uani 1 d . . .
H9 H -0.2519 1.0767 0.7150 0.033 Uiso 1 calc . . R
C12 C 0.6312(16) 0.6335(16) 0.2093(12) 0.020(3) Uani 1 d . . .
C15 C 0.6904(18) 0.7491(18) 0.3013(15) 0.030(4) Uani 1 d . . .
H15 H 0.7922 0.7885 0.3040 0.036 Uiso 1 calc . . R
C17 C -0.0351(18) 0.8949(17) 0.8432(14) 0.028(3) Uani 1 d . . .
H17 H -0.0314 0.8597 0.9042 0.033 Uiso 1 calc . . R
C20 C 0.0892(16) 0.8643(16) 0.7750(13) 0.023(3) Uani 1 d . . .
H20 H 0.1753 0.8117 0.7911 0.028 Uiso 1 calc . . R
C22 C 0.4833(18) 0.5776(18) 0.2101(13) 0.027(3) Uani 1 d . . .
H22 H 0.4439 0.4986 0.1509 0.033 Uiso 1 calc . . R
C24 C 0.0799(17) 0.9144(16) 0.6837(13) 0.024(3) Uani 1 d . . .
C26 C 0.3869(17) 0.6332(17) 0.2961(14) 0.025(3) Uani 1 d . . .
H26 H 0.2858 0.5924 0.2932 0.030 Uiso 1 calc . . R
C30 C 0.5981(18) 0.8067(18) 0.3898(15) 0.029(3) Uani 1 d . . .
H30 H 0.6394 0.8824 0.4509 0.035 Uiso 1 calc . . R
C33 C 0.4450(16) 0.7494(16) 0.3850(13) 0.021(3) Uani 1 d . . .
C2AA C -0.461(2) 0.955(3) 0.8386(17) 0.053(6) Uani 1 d . . .
H2AA H -0.5399 0.9753 0.8903 0.080 Uiso 1 calc . . GR
H2AB H -0.4582 0.8517 0.8059 0.080 Uiso 1 calc . . GR
H2AC H -0.4885 0.9996 0.7814 0.080 Uiso 1 calc . . GR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S2 Tl2 S4 87.65(11) . 2_566 ?
P5 S2 Tl2 88.57(18) . . ?
P5 S4 Tl2 109.84(19) . 2_566 ?
S2 P5 S4 116.4(2) . . ?
O3 P5 S2 112.5(5) . . ?
O3 P5 S4 110.9(4) . . ?
O10 P5 S2 111.2(4) . . ?
O10 P5 S4 111.3(5) . . ?
O10 P5 O3 92.0(6) . . ?
C24 O3 P5 122.1(9) . . ?
C8 C5 C1 108.7(14) . . ?
C12 C5 C8 112.8(14) . . ?
C12 C5 C1 113.7(14) . . ?
C33 O10 P5 125.6(9) . . ?
C2 C4 C0AA 108.6(13) . . ?
C2 C4 C2AA 110.9(16) . . ?
C2AA C4 C0AA 112.1(13) . . ?
C9 C0AA C4 120.3(13) . . ?
C9 C0AA C17 117.4(14) . . ?
C17 C0AA C4 122.3(14) . . ?
C24 C1AA C9 118.2(14) . . ?
C0AA C9 C1AA 122.3(15) . . ?
C15 C12 C5 119.2(13) . . ?
C22 C12 C5 123.4(14) . . ?
C22 C12 C15 117.3(14) . . ?
C12 C15 C30 121.1(14) . . ?
C0AA C17 C20 122.2(14) . . ?
C24 C20 C17 118.1(13) . . ?
C12 C22 C26 123.2(15) . . ?
C1AA C24 O3 117.9(13) . . ?
C1AA C24 C20 121.8(13) . . ?
C20 C24 O3 120.1(13) . . ?
C33 C26 C22 118.9(14) . . ?
C33 C30 C15 119.5(16) . . ?
O10 C33 C26 123.2(13) . . ?
O10 C33 C30 116.7(14) . . ?
C26 C33 C30 119.9(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl2 S2 2.986(4) . ?
Tl2 S4 3.110(4) 2_566 ?
S2 P5 1.957(5) . ?
S4 Tl2 3.110(4) 2_566 ?
S4 P5 1.973(5) . ?
P5 O3 1.634(11) . ?
P5 O10 1.621(11) . ?
C2 C4 1.49(2) . ?
O3 C24 1.388(17) . ?
C5 C8 1.52(2) . ?
C5 C1 1.55(2) . ?
C5 C12 1.50(2) . ?
O10 C33 1.377(17) . ?
C4 C0AA 1.54(2) . ?
C4 C2AA 1.54(2) . ?
C0AA C9 1.37(2) . ?
C0AA C17 1.39(2) . ?
C1AA C9 1.41(2) . ?
C1AA C24 1.37(2) . ?
C12 C15 1.40(2) . ?
C12 C22 1.36(2) . ?
C15 C30 1.41(2) . ?
C17 C20 1.40(2) . ?
C20 C24 1.37(2) . ?
C22 C26 1.41(2) . ?
C26 C33 1.38(2) . ?
C30 C33 1.39(2) . ?
